Dimethylformamide → 1-Hydroxy-3-(2,2,2-trifluoroethylthio)-prop-2-ene
反応式
[F:1][C:2]([F:6])([F:5])[CH2:3][SH:4].[CH2:7]([OH:10])[C:8]#[CH:9].[OH-].[K+].CN(C)C=O>O>[OH:10][CH2:7][CH:8]=[CH:9][S:4][CH2:3][C:2]([F:6])([F:5])[F:1]参加物
6
実験手順
A mixture of 2.32 g 2,2,2-trifluoroethanethiol, 1.12 prop-2-yne-1-ol, 300 mg potassium hydroxide and 40 ml dimethylformamide is stirred at ambient temperature for 20 hours. The mixture is poured into 150 ml of water and extracted with 100 ml ethyl acetate (3 times). The organic phase is washed with water, dried and concentrated. The crude product is purified by column chromatography to obtain 75 mg of pure 1-hydroxy-3-(2,2,2-trifluoroethylthio)-prop-2-ene.
後処理
- extractionextracted with 100 ml ethyl acetate (3 times)
- washThe organic phase is washed with water
- customdried
- concentrationconcentrated
- customThe crude product is purified by column chromatography
出典と根拠
- ORDレコード
- ord-a4e31eede09542dc982fa294b47e544c
- 出典データセット
- uspto-grants-2003_03
- 特許番号
- US06534447B1
反応ノート
読み込み中…